β-SiC粉体Si杂质的亚临界水热去除工艺

硅酸盐通报 ›› 2021, Vol. 40 ›› Issue (2): 591-596.

所属专题：陶瓷

β-SiC粉体Si杂质的亚临界水热去除工艺

王波^1,2, 段晓波^1,2,3, 邓丽荣^1,2,3, 陆树河^1,2,3, 王晓刚^1,2,3, 白枭^1,2

1.西安科技大学材料科学与工程学院,西安 710000;
2.陕西省硅镁产业节能与多联产工程技术研究中心,西安 710000;
3.咸阳新能源材料产业技术研究院,咸阳 712000

收稿日期:2020-10-13 修回日期:2020-11-25 出版日期:2021-02-15 发布日期:2021-03-10
通讯作者: 段晓波,博士,讲师。E-mail:xiaobo12558@163.com
作者简介:王波(1995—),男,硕士研究生。主要从事高纯碳化硅粉体的研究。E-mail:waangb@qq.com
基金资助:
国家自然科学基金青年项目(51602254);陕西省自然科学基础研究计划(2020JQ-737);咸阳市重大科技专项计划(2019K01-13)

Subcritical Hydrothermal Removal of Si Impurity in β-SiC Powder

WANG Bo^1,2, DUAN Xiaobo^1,2,3, DENG Lirong^1,2,3, LU Shuhe^1,2,3, WANG Xiaogang^1,2,3, BAI Xiao^1,2

1. College of Materials Science and Engineering, Xi'an University of Science and Technology, Xi'an 710000, China;
2. Shaanxi Engineering Research Center of Energy Saving and Polygeneration in Silicon and Magnesium Industry, Xi'an 710000, China;
3. Xianyang Industrial Technology Research Institute of New Energy Materials, Xianyang 712000, China

Received:2020-10-13 Revised:2020-11-25 Online:2021-02-15 Published:2021-03-10

摘要/Abstract

摘要： 选用多热源法合成的β-SiC粉体为原料,采用亚临界水热法去除β-SiC粉体中的含Si杂质。通过XRD、SEM、EDS及可见分光光度计等对β-SiC粉体的物相组成、微观结构及Si杂质含量进行表征,重点研究β-SiC粉体中含Si杂质的亚临界水热去除工艺参数优化。结果表明,β-SiC粉体中的含Si杂质主要为SiO₂和游离硅(F·Si),而F·Si主要以大颗粒的形式存在。反应浓度增大、反应时间延长和反应温度升高均有利于提高Si杂质的去除率。最佳水热法处理工艺为:液固比5∶2,NaOH浓度4 mol·L^-1,反应温度180 ℃,反应时间4 h。在此工艺下,β-SiC粉体中SiO₂的去除率达到100%,F·Si的去除率为96.4%。

关键词: β-SiC粉体, 水热法, 碱处理, Si杂质, 提纯

Abstract: The β-SiC powder synthesized by the multi-heat source method was selected as the raw material, and the Si impurity in the β-SiC powder were removed by the subcritical hydrothermal method. The phase composition, microstructure and Si impurity content of β-SiC powder were characterized by XRD, SEM, EDS and visible spectrophotometer, and focused on the optimization of subcritical hydrothermal removal process parameters for Si impurity in β-SiC powder. The results show that the Si impurities in β-SiC powder are mainly SiO₂ and free silicon (F·Si), while the F·Si mainly existe in the form of large particles. The increase of reaction concentration, reaction time and reaction temperature have beneficial to improve the removal rate of Si impurities. The best hydrothermal treatment process is as follows: the liquid-solid ratio is 5∶2, the NaOH concentration is 4 mol·L^-1, the best reaction temperature is 180 ℃, and the best reaction time is 4 h. Under this process, the removal rate of SiO₂ in β-SiC powder reaches 100%, and the removal rate of F·Si is 96.4%.

Key words: β-SiC powder, hydrothermal method, alkali treatment, Si impurity, purification

中图分类号:

TQ163

王波, 段晓波, 邓丽荣, 陆树河, 王晓刚, 白枭. β-SiC粉体Si杂质的亚临界水热去除工艺[J]. 硅酸盐通报, 2021, 40(2): 591-596.

WANG Bo, DUAN Xiaobo, DENG Lirong, LU Shuhe, WANG Xiaogang, BAI Xiao. Subcritical Hydrothermal Removal of Si Impurity in β-SiC Powder[J]. BULLETIN OF THE CHINESE CERAMIC SOCIETY, 2021, 40(2): 591-596.

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β-SiC粉体Si杂质的亚临界水热去除工艺

Subcritical Hydrothermal Removal of Si Impurity in β-SiC Powder

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